|Publication number||US7128945 B2|
|Application number||US 10/214,788|
|Publication date||Oct 31, 2006|
|Filing date||Aug 8, 2002|
|Priority date||Aug 10, 2001|
|Also published as||DE10139553A1, DE10139553B4, US20030047033|
|Publication number||10214788, 214788, US 7128945 B2, US 7128945B2, US-B2-7128945, US7128945 B2, US7128945B2|
|Inventors||Gerd Scheying, Thomas Brinz|
|Original Assignee||Robert Bosch Gmbh|
|Export Citation||BiBTeX, EndNote, RefMan|
|Patent Citations (10), Classifications (27), Legal Events (6)|
|External Links: USPTO, USPTO Assignment, Espacenet|
The present invention relates to a method of producing a material library from surface areas having different properties.
Conventional sputtering methods, among others, are used in combinatory chemistry for the synthesis of single-phase and multiphase surface systems, where materials of different chemical compositions are applied to a disk-shaped substrate, for example, a wafer, using an automated process known as high-throughput process. In this manner, surface systems having a plurality of areas with different surface compositions may be manufactured. The individual areas may be characterized regarding their physical and/or chemical properties by customary analytical methods, so that the surface composition best suited for the given application may be selected from among the differing and separately situated areas.
Conventionally, a sol/gel method for the synthesis of ceramic or metallic single-phase or multiphase systems. In this method different salts and salt mixtures are used as precursors, for example, and are converted to the desired coating materials using a sol/gel process. The sol/gel is then applied, using a dispensing process, to a substrate, which may be manufactured from a ceramic material. By applying different sols/gels in areas separated from one another, a combinatory library is produced, which may be evaluated analytically for its physical and/or chemical properties.
The method according to the present invention for producing a material library from surface areas having different properties, in which at least two suspensions are mixed for producing the mixtures, has the advantage that, by using suspensions, mixtures of materials which were not applicable for this purpose in processes such as the sol/gel process are also usable for producing a combinatory library. Thus, in the exemplary method according to the present invention, mixtures of metals, ceramics, and/or plastics, each present in a suspension, may be producible. By using single-component suspensions, any desired mixture may be produced from an unlimited number of materials.
In the exemplary method according to the present invention, which may be used in particular for mixing solid materials, a plurality of surface systems is produced, which form the combinatory library and are analyzable regarding their physical and/or chemical properties.
The exemplary method according to the present invention may be well suited for producing single-phase or multiphase surface systems. For example, a precious metal phase and a precious metal/ceramic phase may be present side-by-side.
The suspensions used according to an exemplary embodiment of the present invention may be present in any desired form. The suspensions may be liquid or almost solid, i.e., a paste, and may be homogeneously and thoroughly mixed in this state using appropriate equipment.
The term “suspension” may be understood in its broadest sense, i.e., any type of solids dispersed in any type of fluid are included. The suspension represents a stable disperse system, i.e., the solid particles are insoluble or only slightly soluble and do not or only slightly agglomerate in the solvent. Organic solvents or aqueous solvents may be used as the fluid, for example.
The solvents of the at least two suspensions may be the same or different. If they are of the same type, the suspensions and the mixtures may be jointly produced therefrom by introducing at least two different precursors in different, defined concentrations into a solvent, so that mixtures representing mixed suspensions are obtained. The mixtures thus obtained are applied to the substrate.
The substrate used in an exemplary method according to the present invention may be produced from a metallic material or a ceramic material or also from any desired material suited to the application at hand.
According to an exemplary embodiment of the method according to the present invention, a powdery precursor is used for producing the suspensions. The precursor may be a metallic compound or a semimetallic compound or a plastic. In particular, metallic or semimetallic oxidic or nitridic compounds are well suited for the exemplary method according to the present invention.
The particle size of the powdery precursors is between about 5 Å and about 10,000 Å, for example.
The use of mixtures, dopings, alloys, and/or blends of metals and/or plastics as precursors, i.e., for the production of the mixtures, is also possible.
As an example of a paste-like suspension, a plastic composite which represents a kind of thermoplastic may be softened and then mixed with another suspension. Other examples of suspensions include ceramic/metallic composites and metallic oxides.
Chemical reactions may occur between the precursors present in the individual suspensions. However, chemical reactions may also occur between the substrate and the mixtures applied thereto.
Furthermore, the mixtures applied and the substrate made of a ceramic material may adhere to one another after the material library has been produced.
According to an exemplary embodiment of a combinatory method, the suspensions are mixed using automated means.
If the surface system to be produced is to be a porous system, one of the at least two suspensions may represent a pore-forming suspension. For example, a pore-forming suspension may be carbon particles in an organic matrix, which may be burned off in a subsequent heat treatment. By using discrete amounts of such pore formers, the micromorphology of the surface systems produced may be adjusted in a controlled manner.
The combinatory system present after the application of the mixtures to the substrate may be subjected to a post-treatment. Thus, the combinatory system may be treated, for example, by post-treatment processes known as sintering processes. The combinatory system may be sintered, for example, at a defined temperature under a defined atmosphere and/or pressure.
The combinatory system may be heat-treated at a temperature between about 20° C. and about 2000° C., for example. This corresponds to the temperature range used in conventional sintering processes.
The combinatory system may also be exposed to pressure for post-treatment. This pressure may be between about 1 bar and about 20 bar, for example.
Furthermore, the combinatory system may be exposed to a certain gas atmosphere for post-treatment. Thus, when metals are used, the combinatory system may be exposed to a protective atmosphere composed of argon and/or nitrogen. When oxide-ceramic materials are used, air is a suitable atmosphere.
Exposing the combinatory system to a reducing gas atmosphere for post-treatment is also conceivable.
Post-treatment of the combinatory system may be performed in an area-specific manner, i.e., the individual surface areas having different compositions may be post-treated differently, for example, using different pressures and/or temperatures. Wet-chemical post-treatment of the combinatory system is also possible.
The mixtures are expediently applied to the substrate using a dispensing or micro-dispensing method. When using such a method, the mixtures are applicable in defined quantities and degrees of thickness.
The FIGURE shows the sequence of the method according to an exemplary embodiment of the present invention.
In the exemplary method illustrated in the figure, in a first method step, two pasty suspensions are produced from two precursors. A SiO2 powder and an Al2O3 powder are used as precursors. Water is used as the solvent, i.e., as the matrix of the paste-like suspensions. Silicon dioxide and aluminum oxide, respectively, have their thermodynamically stable form in an aqueous matrix, and have their metastable form under standard conditions.
The two pastes present as single-component suspensions are mixed in different proportions in a next method step using a dynamic or static mixer, so that in the present example 64 mixtures of different compositions are obtained. The 64 individual mixtures are applied to a substrate made of ceramic material each in a separate area. The figure shows only 16 of the 64 areas for the sake of clarity.
After the application of the 64 mixtures, a combinatory system is present. In a next step, this combinatory system is subjected to a heat treatment at a temperature of, for example, 500° C. under air atmosphere and normal pressure. After the end of the heat treatment, a combinatory library having 64 different surface systems is present, each of which may be studied using appropriate analytical methods. Depending on the mixing ratios and the subsequent heat treatment, thermodynamically stable mixed phases such as mullite are then formed under certain conditions.
|Cited Patent||Filing date||Publication date||Applicant||Title|
|US5985356||Oct 18, 1994||Nov 16, 1999||The Regents Of The University Of California||Combinatorial synthesis of novel materials|
|US6004617 *||Jun 7, 1995||Dec 21, 1999||The Regents Of The University Of California||Combinatorial synthesis of novel materials|
|US6030917 *||Jul 22, 1997||Feb 29, 2000||Symyx Technologies, Inc.||Combinatorial synthesis and analysis of organometallic compounds and catalysts|
|US6519032 *||Oct 11, 2000||Feb 11, 2003||Symyx Technologies, Inc.||Fiber optic apparatus and use thereof in combinatorial material science|
|US20010039330 *||Dec 12, 2000||Nov 8, 2001||Schunk Stephan Andreas||Combinatorial preparation and testing of heterogeneous catalysts|
|US20020028467 *||Jun 26, 2001||Mar 7, 2002||Hans-Josef Sterzel||Dispensing of suspensions on a microscale for the preparation of material samples in combinatorial materials research, and the testing thereof|
|US20020067120 *||Dec 4, 2000||Jun 6, 2002||General Electric Company||Method for rapid screening of emission-mix using a combinatorial chemistry approach|
|DE10031587A1||Jun 29, 2000||Jan 10, 2002||Basf Ag||Dosierung von Suspensionen im Mikromaßstab zur Herstellung von Materialproben in der kombinatorischen Materialforschung sowie deren Prüfung|
|DE19822077A1||May 16, 1998||Nov 18, 1999||Studiengesellschaft Kohle Mbh||Preparation of library of spatially separted solids by wet-chemical methods on a removable reaction plate, used e.g. to screen for new catalysts or materials|
|DE19955789A1||Nov 19, 1999||May 23, 2001||Basf Ag||Verfahren zur kombinatorischen Herstellung einer Bibliothek von Materialien|
|U.S. Classification||427/245, 427/421.1, 427/383.1, 427/199, 427/195, 427/191, 427/201, 427/197, 427/256, 427/190, 427/243, 427/385.5, 427/331|
|International Classification||B05D3/02, C04B41/87, C04B41/81, C04B41/45, B01J19/00, B05D3/04|
|Cooperative Classification||C04B41/4574, C04B41/87, C04B41/009, B01J19/0046|
|European Classification||C04B41/00V, C04B41/45D2, B01J19/00C, C04B41/87|
|Nov 13, 2002||AS||Assignment|
Owner name: ROBERT BOSCH GMBH, GERMANY
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:SCHEYING, GERD;BRINZ, THOMAS;REEL/FRAME:013500/0477;SIGNING DATES FROM 20021016 TO 20021021
|Sep 18, 2007||CC||Certificate of correction|
|Apr 26, 2010||FPAY||Fee payment|
Year of fee payment: 4
|Jun 13, 2014||REMI||Maintenance fee reminder mailed|
|Oct 31, 2014||LAPS||Lapse for failure to pay maintenance fees|
|Dec 23, 2014||FP||Expired due to failure to pay maintenance fee|
Effective date: 20141031